CN101341102A - Method of refining glass and product obtained - Google Patents

Method of refining glass and product obtained Download PDF

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Publication number
CN101341102A
CN101341102A CNA2006800484662A CN200680048466A CN101341102A CN 101341102 A CN101341102 A CN 101341102A CN A2006800484662 A CNA2006800484662 A CN A2006800484662A CN 200680048466 A CN200680048466 A CN 200680048466A CN 101341102 A CN101341102 A CN 101341102A
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glass
sulfide
equal
oxide
temperature
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CN101341102B (en
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L·茹博
D·马丁
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Saint Gobain Glass France SAS
Compagnie de Saint Gobain SA
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/02—Pretreated ingredients
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/004—Refining agents

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The subject of the invention is a method of refining glass for which the temperature (T log 2) corresponding to a viscosity of 100 poise (10 Pa.s) is greater than or equal to 1480 DEG C., characterized in that sulfides are used as a refining agent. It also relates to the glass article capable of being obtained by this method.

Description

The method of processed glass and the product that obtains
The present invention relates to the processed glass field, especially have the glass of high melt viscosity.
The quality of glass is that glass is given birth to manufacturer, and especially sheet glass is given birth to the main task of top priority of manufacturer, and in each step that glass is made, refining is basic step.This operation comprises the formation of gaseous inclusions of removing all size as far as possible, is called " blister ", bubble or " vesicle ", and their existence in the finished product are controlled by strictness usually and are unacceptable sometimes.Therefore, use (windshield glass especially for automobile, it must provide perfect visibility meter) be strict at the specification of quality aspect making with extra care, and for the application of the sheet glass in the electronic applications, especially as the substrate of flat screens such as liquid-crystal display (LCD) even stricter, the existence of formation of gaseous inclusions may be disturbed electronic operation and/or make some pixel deformation of composing images.
These formation of gaseous inclusions have several sources.The exhaust that they mainly cause from some chemical reaction that takes place during air that captures between powdery substance and the glass melting step.Therefore, carbonate based batch of material (as yellow soda ash, Wingdale or rhombspar) discharges the carbonic acid gas of a large amount of gas form.Formation of gaseous inclusions also may be separated reaction owing to some gas precipitation under certain condition, or owing to melten glass and the chemistry or the electrochemical reaction that are present in some raw material (refractory and/or metal) in the smelting furnace.Formation of gaseous inclusions is trapped in the melten glass body, and they can be therefrom to overflow with square proportional speed of their diameters.Therefore, small bubbles (being called " vesicle " sometimes) only can be overflowed with low-down speed.And owing to the viscosity of glass and the convective motion that bubble may be carried to furnace bottom, the speed that bubble rises may be lowered.
The various process for purification that exist all have the common feature, promptly manage to improve bubble in glass movement rate and/or lower glass in height to shorten the path of bubble air in the smelting furnace.
Usually, following the carrying out of chemical refining operation: be known as the also common compound that adds with batch of material of finishing agent and in melten glass, acutely emit gas, thereby air pocket that forms and small bubbles are assembled and they are carried away to the surface quickly.
Represented soda-lime glass refining of the glass of most industrial-scale production, carried out by means of vitriol usually.Sulfate source, normally sodium sulfate (Na 2SO 4) or gypsum (CaSO 4), adding with batch of material, it at high temperature emits SO when refining beginning 2Gas.The composition of soda-lime glass comprises as follows, represents with weight percent:
SiO 2 60-75％；
B 2O 3 0-5％；
Al 2O 3 0-10％；
MgO 0-8％
CaO 6-15％
Na 2O 10-20%; With
K 2O 0-3％。
Because Na 2The high-content of O and CaO (therefore being expressed as " sodium calcium "), this glass has low-down melt viscosity.
Yet, known when problem be refining when having the glass of high melt viscosity, vitriol is invalid: because its decomposition temperature is low, SO takes place when glass is too sticking 2Gas is emitted.Statement " glass with high melt viscosity " is interpreted as finger, within the scope of the invention, more than or equal to 1480 ℃ glass, such viscosity is necessary to guaranteeing that bubble rises with rational speed corresponding to the temperature (being known as " Tlog2 temperature ") of viscosity of 100 pools.The Tlog2 temperature of above-mentioned sodium calcium compositions only is about 1400 ℃.
Arsenic oxide arsenoxide or weisspiessglanz are normally used for the glass of refining these types, but their shortcoming is toxic.These oxide compounds and the method that forms sheet glass in addition, it is incompatible to be known as " float glass process ", and described float glass process is melten glass is poured on the molten tin bath.
Recently, proposed to use stannic oxide as finishing agent, the latter and float glass process are compatible.
The purpose of this invention is to provide a kind of improved refining method with glass of high melt viscosity.
For this reason, an object of the present invention is the method for the temperature of refining viscosity corresponding to 100 pools (10Pa.s), it is characterized in that using sulfide as finishing agent more than or equal to 1480 ℃ glass.
This is because the inventor finds with being all beyond one's expectations, and sulfide makes that obtaining very satisfied refining result for the glass with high melt viscosity becomes possibility.
These results are more wonderful, because according to patent documentation US 5 069 826 and US 389 885, soda-lime glass can use sulfide refining, and because their refining mechanism with in addition emit SO when being lower than temperature under the situation of using vitriol 2Relevant.By reading these documents, therefore those skilled in the art can expect that use sulfide can be than using vitriol efficient even lower.Yet, prove as the rest part of this paper, such anything but.
Use this method purified glass advantageously to have more than or equal to 1500 ℃ or 1550 ℃, even 1600 ℃ or even " Tlog2 " temperature of 1650 ℃.
It especially can be:
-being suitable for making the glass composition of the substrate that is used for liquid-crystal display, it comprises following oxide compound, and their weight content changes in following restricted portion:
SiO 2 58-76％；
B 2O 3 2-18％；
Al 2O 3 4-22％；
MgO 0-8％；
CaO 1-12％；
SrO 0-5％；
BaO 0-6%; With
R 2O 0-1% (R 2O refers to alkalimetal oxide),
And more particularly:
SiO 2 58-70％；
B 2O 3 3-15％；
Al 2O 3 12-22％；
MgO 0-8％；
CaO 2-12％；
SrO 0-3％；
BaO＜0.5%; With
R 2O 0-1％，
Perhaps:
SiO 2 58-72％；
TiO 2 0.8-3％；
B 2O 3 2-15％；
Al 2O 3 10-25％；
CaO 2-12％；
MgO 0-3％；
BaO 0-6％；
SrO 0-4％；
ZnO 0-3%; With
R 2O 0-1% (R 2O refers to alkalimetal oxide),
The difference of these compositions and sodium calcium compositions is the unusual alkalimetal oxide of low levels, and their coefficient of expansion is lower than 35 * 10 -7/ ℃, strain point is higher than 650 ℃.The EAGLE that Corning Inc. sells
Figure A20068004846600071
Glass is the example of this class glass;
-have low-expansion glass as the refractory glass window:
SiO 2 78-86％；
B 2O 3 8-15％；
Al 2O 3 0.9-5％；
MgO 0-2％；
CaO 0-1.5％；
Na 2O 0-3%; With
K 2O 0.7％，
The difference of this based composition and sodium calcium compositions is the Na of low levels 2O and CaO, the example are that Corning Inc. sells
Figure A20068004846600072
Glass;
-can be used as the glass of the substrate of the display screen that is known as " plasma body " screen, it has following composition especially, and itself and sodium calcium compositions difference are the Na of low levels 2O:
SiO 2 40-75％；
Al 2O 3 0-12％；
Na 2O 0-9％；
K 2O 3.5-10％；
MgO 0-10％；
CaO 2-11％；
SrO 0-11％；
BaO 0-17%; With
ZrO 2 2-8％。
Be less than or equal to 12% according to alkalimetal oxide (especially sodium oxide) content that the inventive method purified glass has usually, or 10%, even 8%, or almost be zero content in some cases.
The sulfide that uses in the context of the invention is advantageously added before the fusion step in the batch of material, and with respect to final glass weight, preferred add-on is more than or equal to 0.05 weight %.Best refining for guaranteeing, this content itself is advantageously more than or equal to 0.1%, or 0.3%, even 0.4%.Do not provide any advantage yet content is too high, and even may change the physical properties of glass sometimes for the quality of final glass.Therefore they are preferably limited to and are less than 2%, even 1%, or 0.8%.
Preferred its corresponding oxide compound forms the sulfide of the part of glass composition, so that the element that can change glass property is not introduced in the use of this sulfide in composition.For example should avoid alkali metalsulphide is incorporated into the composition that can not contain alkalimetal oxide that is used for the LCD substrate.The form of the mixture of the sulfide that used sulfide is can be several different adds.
In the method for the invention, alkali-metal sulfide (Na 2S, K 2S, Li 2S etc.), the sulfide (ZnS, FeS etc.) of sulfide of alkaline-earth metal (CaS, MgS, BaS, SrS etc.) or transition element can use separately or use as mixture.Proved that zinc sulphide (ZnS) is especially suitable, even also be suitable, particularly the zinc sulphide of 0.4-0.6 weight % content for the glass composition that does not contain this oxide compound.
This sulfide also can blast-furnace slag or the form of rich chalcogenide glass powder be provided.
Advantageously vitriol is not joined in the batch of material with sulfide, because observed the reduction of refining quality.
For further improving the refining quality of gained, particularly advantageously be to add the oxide compound of reagent, particularly multivalent element that can the described sulfide of oxidation with sulfide.In these available oxygenants, cerium oxide is for example arranged (with CeO 2Form) or stannic oxide (with SnO 2Form).Arsenic oxide arsenoxide or weisspiessglanz also have this favorable properties, but because their toxicity is not preferred.Consider the color influence of cerium oxide, preferred stannic oxide.These reagent are preferably with respect to final glass weight, more than or equal to 0.1 weight %, or 0.2 weight %, particularly 0.3 weight %, even the weight content of 0.4 weight % adds.Their content preferably is no more than 2%, or 1% or even 0.8%.Under the situation of preferred use stannic oxide (especially when it uses with zinc sulphide), the content of the stannic oxide that is added is preferably 0.4-0.6%.
The inventor found in implementing the process of process for purification of the present invention, and the diameter that may remain in the formation of gaseous inclusions in the glass when finishing the fusion step is residual much bigger when using stannic oxide, arsenic oxide arsenoxide or weisspiessglanz.Therefore these inclusiones can be at an easy rate removed by impelling high temperature to be created in the glass gas of rapid diffusion, for example introduce gas such as helium by bubbling in the melten glass body, and/or by in fusion step forward direction batch of material, adding halogenide such as calcium chloride or magnesium chloride.
Used extraction temperature preferably is less than or equal to 1750 ℃, or 1700 ℃, even 1680 ℃.
Another object of the present invention is to make glass, in particular for the method for the substrate of liquid-crystal display, it comprises the fusion step, according to purification step of the present invention and forming step, and the latter may, for example, be step according to float glass process well known to those skilled in the art.
The method according to this invention is particularly suitable for obtaining various products or goods, and this also is a purpose of the present invention.
By the Tlog2 temperature more than or equal to 1480 ℃, especially 1500 ℃ or 1550 ℃, or even 1600 ℃ glass obtain such goods, its feature particularly in, the sulphur content that its chemical composition comprises, the SO of the umber with per 1,000,000 (ppm) 3Expression, more than or equal to 40ppm, or even the fact of 60ppm (promptly with respect to final glass, 0.004 or 0.006 weight %).Described sulphur content is less than usually or equals 0.5%, or 0.2%, even 0.1%.
Known to the inventor, still the process for purification that does not have to use or describe any type of sulphur of use is used to produce the glass with high melt viscosity, especially be applicable to the substrate of liquid-crystal display, thereby still do not describe the substrate that in its composition, contains the sulphur of such amount.
And what shown is that the preferred embodiment that stannic oxide uses with sulfide is particularly suitable for obtaining other new favourable goods.
More than or equal to 1480 ℃, especially 1500 ℃, even 1600 ℃ glass obtains, and comprise stannic oxide in its composition, it is characterised in that [Sn to these goods by the Tlog2 temperature 2+The Sn that]/[is total] ratio is more than or equal to 0.6.
Tin can two kinds of oxidation state be present in the glass: go back ortho states Sn 2+(divalent) and oxidation state Sn 4+(4 valency).[Sn 2+The Sn that]/[is total] ratio (rest part of this paper is represented with the R ratio) be defined as with divalent also ortho states be present in tin in the glass to being present in the mol ratio of all tin in the glass.Therefore high R ratio corresponding to go back ortho states be present in the glass stannic oxide at high proportion.
Known to the inventor, the process for purification of use tin-oxide described in the prior does not have to obtain high like this R ratio.
And the goods of Xian Dinging itself have series of advantages like this, and do not rely on the method that is used to make them.This is because what shown is that the more a high proportion of ortho states tin of going back makes restriction cassiterite SnO 2The danger of crystallization becomes possibility.This special infusible crystalline form can form in stanniferous glass and can destroy glass forming operation owing to producing the crystalline region.In addition, when melten glass contacted with platinum, tin was favourable to go back that ortho states exists mainly.Platinum is because its high-melting-point and high purity usually are used to glass industry.Electrochemical reaction can produce formation of gaseous inclusions in glass yet melten glass contacts with platinum.This is because be dissolved in the water in the glass because the katalysis of platinum can be dissociated into hydrogen (H 2) and oxygen (O 2).The hydrogen that produces is diffused in the platinum, and oxygen is retained in the glass, causes difficult especially small size formation of gaseous inclusions of removing.Therefore, the inventor can prove that tin mainly exists and make to absorb these inclusiones by redox reaction and become possibility to go back ortho states, thereby produces oxygen bubble when having avoided to a great extent contacting with platinum.
Owing to these reasons, advantageously the R ratio is more than or equal to 0.7, or even 0.75 also/or be less than or equal to 0.9, or even 0.85.The glass that has shown gained in these preferred R ratio ranges in addition has best refining quality (therefore minimum formation of gaseous inclusions).This ratio can be by suitable metering SnO 2And the amount of sulfide (particularly ZnS) obtains.Measuring not enough and causing the R ratio under the situation outside this preferable range, also possible is to regulate this R ratio by adding reductive agent (as coke) or oxygenant (as nitrate).
Especially, a kind of preferred goods are the substrates that are used for liquid-crystal display, and its composition comprises following oxide compound, and their weight content changes in following restricted portion:
SiO 2 58-76％；
B 2O 3 2-18％；
Al 2O 3 4-22％；
MgO 0-8％；
CaO 1-12％；
SrO 0-5％；
BaO 0-6%; With
R 2O 0-1％。
Following examples describe the present invention in detail but do not limit it.
A kind of glass composition, it comprises the following oxide compound of the weight content of following qualification, and it begins fusing by batch mixtures and made with extra care 1 hour down at 1650 ℃:
SiO 2 63.8％；
Al 2O 3 16.3％；
B 2O 311.3%; With
CaO 8.5％。
The Tlog2 temperature of glass with this composition is greater than 1650 ℃.
For Comparative Examples C1, do not add finishing agent.Comparative Examples C2, C3 and C4 use respectively 0.2 weight % with gypsum (CaSO 4) stannic oxide (SnO of the form vitriol, 0.5 weight % and the 1 weight % that add 2) refining.
According to the present invention, the method that embodiment 1 implements purification step by use with respect to the zinc sulphide (ZnS) of final glass weight 0.5% weight obtains.For embodiment 2,, in batch mixtures, add the stannic oxide (SnO of equivalent (0.5%) with 0.5% zinc sulphide still according to the present invention 2).In embodiment 2-6, the stannic oxide content that joins in the batch mixtures is made as 0.5 weight %, the content of zinc sulphide in 0.3% (embodiment 3) to changing between 0.8% (embodiment 6).
Following table 1 shown, for each test, and the used zinc sulphide and/or the amount of stannic oxide, by every cm 3Foaming degree that bubbles number is represented and R ratio.The latter passes through
Figure A20068004846600111
Spectrophotometer.
Table 1
ZnS(％) SnO 2(％) Foaming degree (/cm 3) R
C1 - - ＞1000 -
C2 - - 830 -
C3 - 0.5 160 0.25
C4 - 1 30 0.25
1 0.5 - 125 -
2 0.5 0.5 7 0.84
3 0.3 0.5 120 0.6
4 0.4 0.5 60 0.72
5 0.65 0.5 49 1
6 0.8 0.5 65 1
Comparative Examples C1 and C2 show that for this class glass, vitriol is the finishing agent of non-constant, are very insufficient in observed slight improvements aspect the foaming degree.
Embodiment C 3 and C4 show that high quality is refining and can use 1%SnO 2Obtain.
Among the embodiment 1,0.5% sulfide so that zinc sulphide (ZnS) form adds with respect to using vitriol, provides very big improvement.And, observe remaining bubble and have large size, can remove by the minimum prolongation of refining time at an easy rate.Compare with C4 with Comparative Examples C3 and to show that ZnS compares SnO when add fashionablely with same amount 2Even it is more effective
Add 0.5% stannic oxide (SnO with 0.5%ZnS 2) (embodiment 2) have also quite improved refining quality, because the glass that obtains does not almost completely contain the gaseous state inclusion.
What the stannic oxide content for 0.5%, research embodiment 2-6 showed aspect refining quality the best is the zinc sulphide of 0.4-0.6%, more accurate about 0.5% the zinc sulphide of saying.This optimum range and R ratio are that 0.7-0.9, particularly 0.8-0.9 are relevant, and the effect of zinc sulphide is to improve this ratio.Can be pointed out that independent refining (Comparative Examples C3 and C4) with tin only may obtain about 0.25 R ratio.These low R ratios have the risk that increases the cassiterite crystallization and the bubble that produces oxygen when molten glass bath contacts with platinum.
Before with as described in the embodiment, should be understood that those skilled in the art can implement various variants of the present invention as the present invention, and do not exceed the scope of this patent of claims qualification.

Claims (14)

1. the method for a processed glass, described glass more than or equal to 1480 ℃, is characterized in that using sulfide as finishing agent corresponding to the temperature (Tlog2) of the viscosity of 100 pools (10Pa.s).
2. the described method of claim as described above, the Tlog2 temperature of wherein said glass be more than or equal to 1500 ℃, especially 1600 ℃.
3. the described method of one of claim as described above, wherein said glass has the composition that comprises following oxide compound, and their weight content changes in following restricted portion:
SiO 2 58-76％；
B 2O 3 2-18％；
Al 2O 3 4-22％；
MgO 0-8％；
CaO 1-12％；
SrO 0-5％；
BaO 0-6%; With
R 2O 0-1% (R 2O refers to alkalimetal oxide).
4. the described method of one of claim as described above wherein joins described sulfide in the batch of material before the fusion step.
5. the described method of claim as described above, wherein with respect to final glass weight, the add-on of described sulfide is 0.1-0.8 weight %.
6. the described method of one of claim as described above, wherein said sulfide is zinc sulphide (ZnS).
7. the described method of one of claim as described above, wherein add can the described sulfide of oxidation reagent.
8. the described method of claim as described above, wherein said reagent that can sulfide oxidation is the oxide compound of multivalent element.
9. the described method of claim as described above, wherein said reagent that can sulfide oxidation is that stannic oxide is (with SnO 2Form).
10. make glass for one kind, especially for the method for the substrate of liquid-crystal display, it comprises the fusion step, according to the purification step and the forming step of the method for claim 1-9.
11. the described manufacture method of claim as described above wherein adds helium in the melten glass body by bubbling and/or before the fusion step halogenide such as calcium chloride or magnesium chloride is joined in the batch of material.
12. one kind by the Tlog2 temperature more than or equal to the goods that 1480 ℃ glass obtains, the sulphur content of chemical constitution that it is characterized in that it is with SO 3Expression is more than or equal to 0.004%.
13. goods that obtained more than or equal to 1480 ℃ glass by the Tlog2 temperature, its composition comprises stannic oxide, it is characterized in that [Sn 2+The Sn that]/[is total] ratio is more than or equal to 0.6, is preferably 0.7-0.9.
14. as the described goods in one of claim 12 and 13, its composition comprises following oxide compound, their weight content changes in following restricted portion:
SiO 2 58-76％；
B 2O 3 2-18％；
Al 2O 3 4-22％；
MgO 0-8％；
CaO 1-12％；
SrO 0-5％；
BaO 0-6%; With
R 2O 0-1％。
CN2006800484662A 2005-12-22 2006-10-09 Method of refining glass and product obtained Expired - Fee Related CN101341102B (en)

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PCT/FR2006/051002 WO2007074248A1 (en) 2005-12-22 2006-10-09 Method of refining glass and product obtained

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EP1979282A1 (en) 2008-10-15
KR20080083177A (en) 2008-09-16
WO2007074248A1 (en) 2007-07-05
FR2895395B1 (en) 2008-02-22
HK1126467A1 (en) 2009-09-04
FR2895395A1 (en) 2007-06-29
US8168552B2 (en) 2012-05-01
CN101341102B (en) 2011-07-06
US20080269039A1 (en) 2008-10-30

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